WO2021127162A1 - Hydrated ionic clay and tobacco material compositions - Google Patents
Hydrated ionic clay and tobacco material compositions Download PDFInfo
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- WO2021127162A1 WO2021127162A1 PCT/US2020/065587 US2020065587W WO2021127162A1 WO 2021127162 A1 WO2021127162 A1 WO 2021127162A1 US 2020065587 W US2020065587 W US 2020065587W WO 2021127162 A1 WO2021127162 A1 WO 2021127162A1
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- tobacco material
- hydrated ionic
- water
- clay
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Classifications
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
- A24B15/243—Nicotine
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/42—Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/20—Biochemical treatment
Definitions
- Vaporizer devices which can also be referred to as vaporizers, electronic vaporizer devices, e-vaporizer devices or aerosolization devices, can be used for delivery of an aerosol (for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some other gas carrier) containing one or more active ingredients by inhalation of the aerosol by a user of the vaporizing device.
- an aerosol for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some other gas carrier
- an aerosol for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some other gas carrier
- an aerosol for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some other gas carrier
- active ingredients for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some
- Vaporizer devices can be portable, self-contained, and/or convenient for use.
- the user inhales an aerosol, colloquially referred to as “vapor,” which can be generated by a heating element that vaporizes (e.g., causes a liquid or solid to at least partially transition to the gas phase) a vaporizable material, which can be liquid, a solution, a solid, semisolids, a paste, a wax, and/or any other form compatible for use with a specific vaporizer device.
- the vaporizable material used with a vaporizer can be provided within a cartridge (for example, a separable part of the vaporizer device that contains vaporizable material) that includes an outlet (for example, a mouthpiece) for vapor delivery and inhalation of the aerosol by a user.
- a cartridge for example, a separable part of the vaporizer device that contains vaporizable material
- an outlet for example, a mouthpiece
- a typical approach by which a vaporizer device generates an inhalable aerosol from a vaporizable material involves heating the vaporizable material in a vaporization chamber (or a heater chamber) to cause the vaporizable material to be converted to the gas (or vapor) phase.
- a vaporization chamber generally refers to an area or volume in the vaporizer device within which a heat source (e.g., conductive, convective, and/or radiative) causes heating of a vaporizable material to produce a mixture of air and vaporized vaporizable material to form a vapor for inhalation by a user of the vaporization device.
- a heat source e.g., conductive, convective, and/or radiative
- vaporizable materials having a variety of contents and proportions of such contents can be contained in the cartridge.
- Some vaporizable materials may have a smaller percentage of active ingredients per total volume of vaporizable material, such as due to regulations requiring certain active ingredient percentages.
- a user may need to vaporize a large amount of vaporizable material (e.g., compared to the overall volume of vaporizable material that can be stored in a cartridge) to achieve a desired effect.
- nicotine can be extracted from tobacco or other plants and then added to a suitable carrier.
- One such method of extracting nicotine from tobacco is disclosed in U.S. Patent No.
- a humectant such as propylene glycol (PG), vegetable glycerin (VG), or a mixture of PG and VG (PG/V G) to form a vaporizable material.
- PG propylene glycol
- VG vegetable glycerin
- PG/V G a mixture of PG and VG
- the humectant forms a solution with the nicotine and forms an aerosol after vaporization.
- the amount of nicotine in the vaporizable material can be adjusted by adding more or less humectant.
- Other additives can be incorporated into the vaporizable material such as flavorings.
- liquid vaporizable materials suitable for use in electronic vaporizer devices can be prepared by inclusion of one or more of the features described herein or comparable/equivalent approaches as would be understood by one of ordinary skill in the art.
- aspects of the current subject matter relate to methods and systems extracting nicotine from tobacco or other plant material and preparing liquid vaporizable materials.
- a method of extracting nicotine from tobacco material and directly into a liquid vaporizable material is described.
- one or more of the following features may optionally be included in any feasible combination.
- a composition including a hydrated ionic clay and a tobacco material is disclosed.
- a device comprising a heating element configured to heat the composition of any one of the preceding claims to deliver nicotine or a salt thereof to a user.
- a method of extracting nicotine is disclosed. The method of extracting nicotine from tobacco material includes contacting tobacco material with hydrated ionic clay to form a composition, and contacting the composition with a solvent to extract the nicotine from the tobacco material.
- a method of extracting nicotine is disclosed.
- Tobacco material is ground to form powdered tobacco material.
- Ionic clay is mixed with a first amount of water to form a first dispersion.
- the powdered tobacco material is mixed with the first dispersion to form a second dispersion.
- a portion of the first amount of water from the second dispersion is evaporated to form a loose cake.
- the loose cake is compressed to form a pellet.
- the pellet is immersed in a first solution including a glycol and a glycerol.
- a second amount of water is added to the first solution to form a second solution, the second solution containing the nicotine extracted from the pellet.
- a method of manufacturing a pellet containing tobacco material includes grinding tobacco material to form a powdered tobacco material.
- a hydrated ionic clay is mixed with a first amount of water to form a first dispersion.
- the powdered tobacco material is mixed with the first dispersion to form a second dispersion.
- a portion of the first amount of water is evaporated from the second dispersion to form a loose cake.
- the loose cake is compressed to form the pellet containing tobacco material.
- the tobacco formulation comprising hydrated ionic clays, optionally formulated with humectants such as vegetable glycerin and glycols, organic acids, flavoring agents including both natural and artificial, is subjected to temperatures in the 100 °C to 400 °C range, preferably in 150 °C to 300 °C range, to generate a vapor.
- humectants such as vegetable glycerin and glycols, organic acids, flavoring agents including both natural and artificial
- FIG. 1 illustrates a graph of the thermal stability of hydrated ionic clays and Burley tobacco.
- FIG. 2 illustrates a tobacco leaf coated with hydrated ionic clay.
- FIG. 3 illustrates a tobacco powder and hydrated ionic clay composition.
- FIG. 4 shows a plurality of pellets formed from powdered tobacco material and hydrated ionic clay.
- FIG. 5A shows pellet in a PG/V G/water solution at 0 hours.
- FIG. 5B shows pellet in a PG/V G/water solution after about 24 hours.
- FIG. 6 presents a table of pH data for multiple chemicals and compositions.
- FIG. 7 is a graph presenting the percent of nicotine extracted for Examples 1, 2, and 3 at room temperature.
- FIG. 8 is a graph presenting the percent of nicotine extracted for Example 4 at a temperature of 70 °C.
- FIG. 9 is a graph presenting the percent of nicotine extracted into solution of PG/V G for several grades of Laponite at room temperature and 70 °C.
- FIG. 10 is a graph presenting the percent of nicotine vaporized for Examples 6 and 7 at a temperature of 200 °C.
- Implementations of the current subject matter include compositions and methods of preparing hydrated ionic clay and tobacco material compositions.
- the hydrated ionic clay and tobacco material compositions can be formed into a mass, such as a pellet, sheet, brick, bead, tablet, powder, semi-solid, loose cake, granulation, free flowing powder, plug, cylinder, porous rod, or other suitable shape including hollow forms with various porous structures or a coating.
- hydrated ionic clay and tobacco material compositions are in a form of a loose, powdered mixture of the hydrated ionic clay and the powdered tobacco material.
- Implementations of the current subject matter also include systems and methods of extracting active ingredients (e.g.
- vaporizable materials that may be liquid, a solution, a solid, semi-solid, loose cake, a wax, or other form as may be compatible with use of a specific vaporizer device.
- the vaporizable material is a liquid comprising nicotine and a humectant that is vaporized and forms an aerosol using a vaporizer.
- Vaporizer is used generically in the following description to refer to a vaporizer device. Examples of vaporizers consistent with implementations of the current subject matter include electronic vaporizers, combustible vaporizers, or the like. Such vaporizers are generally portable, hand-held devices that heat a vaporizable material to provide an inhalable dose of the vaporizable material.
- the vaporizable material used with a vaporizer may optionally be provided within a cartridge (e.g., a part of the vaporizer that contains the vaporizable material in a reservoir or other container and that can be refillable when empty or disposable in favor of a new cartridge containing additional vaporizable material of a same or different type).
- a vaporizer may be a cartridge-using vaporizer, a cartridge-less vaporizer, or a multi-use vaporizer capable of use with or without a cartridge.
- a multi-use vaporizer may include a heating chamber (e.g., an oven) configured to receive a vaporizable material directly in the heating chamber and also to receive a cartridge or other replaceable device having a reservoir, a volume, or the like for at least partially containing a usable amount of vaporizable material.
- a heating chamber e.g., an oven
- a cartridge or other replaceable device having a reservoir, a volume, or the like for at least partially containing a usable amount of vaporizable material.
- a liquid vaporizable material e.g., a carrier solution in which an active and/or inactive ingredient(s) are suspended or held in solution or a neat liquid form of the vaporizable material itself
- a liquid vaporizable material can likewise be capable of being completely vaporized or can include some part of the liquid material that remains after all of the material suitable for inhalation has been consumed.
- nicotine is extracted from tobacco material into a humectant.
- nicotine is extracted directly from tobacco material (e.g. powdered tobacco within the hydrated ionic clay and tobacco composition), and into solution with a humectant such as a PG/VG mixture.
- the nicotine extraction process avoids the need for a separate extraction process to obtain the nicotine, which would in turn be added into a humectant.
- Natural extraction of nicotine, alkaloids, and flavoring agents directly into PG/VG may eliminate the need for formulating an e-liquid with synthetic nicotine and flavoring agents. Additional flavors or additives to customize the extractant formulation can be added, if required.
- Implementations according to the present process also avoid the need for subsequent purification of a tobacco material extract to obtain the nicotine, which may be required step for other extraction processes. Implementations according to the present process also avoid the use of harsh or toxic chemicals that can contaminate the nicotine and ultimately the vaporizable material.
- Implementations according to the present process also avoid the need for high temperature extraction processes, or high temperature purification processes, since the nicotine can be extracted from the tobacco material at standard conditions (i.e. room temperature, standard pressure). Without being bounded to any particular theory, it is believed that implementations according to the present process selectively extract nicotine/alkaloids from a tobacco material while avoiding the extraction of undesirable, higher molecular weight compounds, as compared to other extraction processes.
- Various implementations include the release of nicotine at lower temperatures into a vapor form.
- Various implementations include permeating water into a tobacco structure for migration of nicotine/alkaloids.
- Various implementations include release of nicotine in final product in the pH range of 5 to 8.
- Various implementations include release of nicotine from tobacco into a gel matrix.
- Various implementations include release of nicotine into viscous liquids or semi solids or hydrogels.
- Various implementations include pre-heating of the product to improve nicotine release efficiency at low temperatures.
- Various implementations include use of clays as binders to modify the bulk density, rod density, porosity, flow properties, compressibility, thermal conductivity, form factors, moldability, processability, and manufacturability of a composition.
- compositions comprising a thermally stable clay and like materials, which optionally do not release any organic materials below 300 °C.
- Various implementations enable multiple heating element designs and form factors to make it compact and energy efficient.
- Various implementations include wetting agents or humectants along with ionic clays.
- Implementations according to the present disclosure are suitable for industrial scale extraction of nicotine from tobacco material. Implementations according to the present disclosure are suitable for in situ extraction of nicotine from tobacco material within a personal-sized, vaporization device.
- a hydrated ionic clay is added to the tobacco material.
- the hydrated ionic clay in the hydrated ionic clay and tobacco material composition facilitates an nicotine exchange process that allows nicotine to be released from the tobacco material.
- nicotine is released from the tobacco material and migrates to a surface of a tobacco material/hydrated ionic clay matrix.
- the nicotine may be stabilized on the surface of the matrix by hydrogen bonding and/or ionic bonding.
- tobacco/hydrated ionic clay create acid/base junction in solid phase or pH gradient, and it is possible that the presence of polar solvents such as water could transport nicotine to the intersection of tobacco/ hydrated ionic clay from the interior of tobacco.
- the nicotine can be extracted into a humectants to form e-liquids, or heated (optionally in presence of humectants) to form an aerosol containing nicotine.
- the nicotine transport process occurs within the tobacco material/hydrated ionic clay matrix.
- bound nicotine is converted to free base nicotine.
- protonated and freebase nicotine may exist in equilibrium, and that the composition of each formed inside tobacco is governed by the localized pH.
- the equilibrium of protonated and freebase nicotine dynamically change or switch based on environmental conditions of the tobacco material/hydrated ionic clay matrix and temperature.
- Increasing the temperature increases the rate of nicotine release from tobacco material/hydrated ionic clay matrix, as well as increasing the rate of extraction of the nicotine into the humectant.
- the addition of water can facilitate the nicotine/ion exchange process and release of nicotine to the surface of the matrix.
- the addition of water can also facilitate the release of nicotine from the tobacco material at lower temperatures as compared to the absence of added water.
- the mobility of the nicotine release may be impacted by structured water versus free water differently.
- the composition comprises a hydrated ionic clay and a tobacco material.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 4 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 2 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay in an amount between 0.1 wt% to 5 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay in an amount between 0.1 wt% to 10 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 99 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 90 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 80 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 70 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 60 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 40 wt% to 50 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 50 wt% to 90 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 50 wt% to 80 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 50 wt% to 70 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 50 wt% to 60 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 80 wt% to 99 wt% of the composition, and any subranges therebetween.
- the composition can comprise the tobacco material in an amount between 90 wt% to 99 wt% of the composition, and any subranges therebetween.
- the composition further comprises water.
- the composition can comprise the water in an amount between 5 wt% to 50 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 5 wt% to 40 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 5 wt% to 30 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 5 wt% to 20 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 5 wt% to 15 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 10 wt% to 40 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 10 wt% to 30 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 10 wt% to 20 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 10 wt% to 15 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 1 wt% to 10 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 0.1 wt% to 10 wt% of the composition, and any subranges therebetween.
- the composition can comprise the water in an amount between 2 wt% to 6 wt% of the composition, and any subranges therebetween.
- the composition can comprise the hydrated ionic clay and the tobacco material in any of the aforementioned amounts, except in combinations where such amounts are mutually exclusive.
- the composition can comprise the hydrated ionic clay, the tobacco material, and water in any of the aforementioned amounts, except in combinations where such amounts are mutually exclusive.
- the composition comprises a hydrated ionic clay, a tobacco material, and water.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt%, the tobacco material in an amount between 40 wt% to 99 wt%, and the water in an amount between 5 wt% to 50 wt% of the composition.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 4 wt%, the tobacco material in an amount between 50 wt% to 90 wt%, and the water in an amount between 5 wt% to 40 wt% of the composition.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 3 wt%, the tobacco material in an amount between 60 wt% to 90 wt%, and the water in an amount between 5 wt% to 30 wt% of the composition.
- the composition can comprise the hydrated ionic clay in an amount between 1 wt% to 3 wt%, the tobacco material in an amount between 50 wt% to 90 wt%, and the water in an amount between 10 wt% to 30 wt% of the composition.
- the hydrated ionic clay is a synthetic layered material carrying either a negative charge or a positive charge.
- the hydrated ionic clay can be an anionic layered alkaline clay.
- the hydrated ionic clay can comprise silicates.
- the hydrated ionic clay can comprise alkali and/or alkaline earth metal silicates.
- the hydrated ionic clay can be a magnesium silicate clay.
- the hydrated ionic clay can be a sodium magnesium silicate clay.
- the hydrated ionic clay can be a synthetic trioctahedral clay mineral.
- the hydrated ionic clay comprises aluminates, titanates and/or zirconates.
- the hydrated ionic clay can be an aluminate, such as layered double hydroxide carrying net positive charge.
- the hydrated ionic clay can be a synthetic phyllosilicate.
- the synthetic phyllosilicate can be a lithium magnesium sodium orthosilicate.
- the hydrated ionic clay can comprise phosphates.
- the synthetic phyllosilicate can be an inorganic composition comprising hydrogen, lithium, magnesium, sodium, oxygen, and silicon.
- the inorganic composition is dilithium;hexadecamagnesium;disodium;l,3,5,7-tetraoxido-2,4,6,8,9,10-hexaoxa-l,3,5,7- tetrasilatricyclo[3.3.1.13,7]decane;dodecahydroxide.
- the hydrated ionic clay can include an additive within the clay matrix.
- the hydrated ionic clay can be Laponite.
- Laponite also known as hectorite, is a synthetic, colloidal, layered silicate manufactured from naturally occurring minerals. Laponite, an inorganic polymer, has higher gelling strength and can hold more tobacco material than natural clays. Laponite is available in multiple different grades.
- the hydrated ionic clay is a gel forming grade, e.g. a gel forming grade of Laponite.
- the hydrated ionic clay is a gel forming grade, e.g. a sol forming grade of Laponite.
- Water can be added to the ionic clay to form a hydrated ionic clay.
- a portion of the water in the hydrated ionic clay can be bound within the crystalline lattice, with any excess water being free moisture.
- the hydrated ionic clay may have a surface hydroxyl concentration contributing to localized negative charges.
- Other moieties including silicon oxides may also contribute to the hydrated ionic clay’s anionic properties.
- Mg2+, Li+, K+, and Na+ ions may contribute to a localized positive charges, and also serve as exchangeable cations for the hydrated ionic clay.
- the charged nature and the interlayer space within the hydrated ionic clay can provide for adsorption of organic molecules.
- the tobacco material includes one or more types of tobacco.
- the tobacco material can be a single type of tobacco or a blend. Any variety of tobacco can be used including, but not limited to, Aromatic Fire-cured, Brightleaf, Burley, Cavendish, Corojo, Criollo, Dokha, Ecuadorian Sumatra, Habano, Kasturi, Latakia, Maduro, Oriental, Perique, Shade, Thuoc lao, Type 22, Virginia, White Burley, Wild, Yl, and the like.
- the tobacco material may be dry-ice expanded tobacco (DIET), Hue-cured tobacco, and/or air- cured tobacco.
- the composition is contained within a cartridge.
- the composition is heated in a device comprising a heating element configured to heat the composition to deliver nicotine or a salt thereof to a user.
- the device can be an electronic nicotine delivery system.
- FIG. 1 shows a graph of the thermal stability of two grades of Laponite and Burley tobacco material.
- the initial weight loss at 100 °C of the Laponite is attributable to the loss of the free water. In all, the Laponite loses less than about 10% of its weight up to 600 °C, with almost all of the weight loss being water. On the other hand, tobacco loses 60 % of its weight before reaching 400 °C. Hydrated ionic clays, such as Laponite, are non-flammable and thermally stable at temperatures below 800 °C.
- the hydrated ionic clay (e.g. Laponite) is gel forming grade the forms a high viscosity colloidal dispersion with water.
- the hydrated ionic clay is sol forming grade the forms a low viscosity colloidal dispersion with water. While the actual viscosity of the colloidal dispersion depends on the amount of hydrated ionic clay used in the dispersion, the aforementioned high and low viscosity descriptors refer to relative viscosities at a given concentration.
- Laponite forms an alkaline dispersion that has a basic pH value, with many of the dispersions having a pH value between 9 and 10. It is believed that all grades of Laponite that have a basic pH can be used in the formulation. However, Laponites could be stabilized to neutral or lower pH by adding acids, for example, to create dispersions having a final pH value of the range from 5 to 12.
- the acids can be organic acids such as carboxylic acids or inorganic acids such as phosphoric acid.
- the tobacco leaves are dried or cured to remove excess moisture and break down chemical compounds.
- Methods of drying or curing tobacco material include air drying, oven drying, flame-curing, convective drying, vacuum drying, free drying, and combinations thereof. Any type of tobacco material is generally suitable for use according the methods and systems disclosed herein.
- the tobacco material is a Burley tobacco.
- the hydrated ionic clay is hydrated.
- a quantity of hydrated ionic clay is measured and added to warm water.
- the water may be heated to a temperature of 40 °C to 80 °C. Heating the water helps the rate at which the hydrated ionic clay disperses in the water.
- the composition can be mixed by stirring until a uniform dispersion is achieved.
- whole tobacco leaves are coated with hydrated ionic clay as shown in FIG. 2.
- Coating the whole tobacco leaf can be completed before or after the aforementioned drying process.
- the hydrated ionic clay coating can be applied by a spraying process, contact process (e.g. brushing) or by dipping the leaf in a hydrated ionic clay dispersion.
- Coating the tobacco leaf with hydrated ionic clay prior to a drying or curing process can avoid multiple drying steps and facilitate the breakdown of chemical compounds.
- Coating the whole tobacco leaf with hydrated ionic clay can also be accomplished a minimal need for capital investment in equipment.
- the tobacco leaf After coating with the hydrated ionic clay, the tobacco leaf can be rolled, cut, pulverized, and/or ground into a powder.
- a method of manufacturing a pellet (or other compressed form) containing tobacco material comprises grinding tobacco material to form a powdered tobacco (particle size distribution may range from 50 to 5000 microns) material, mixing a hydrated ionic clay with a first amount of water to form a first dispersion, mixing the powdered tobacco material with the first dispersion to form a second dispersion, evaporating a portion of the first amount of water from the second dispersion to form a loose cake, and compressing the loose cake to form the pellet containing tobacco material.
- the tobacco leaves are ground to form a powdered tobacco material.
- the tobacco leaves coated with hydrated ionic clay are ground to form a powdered tobacco material and hydrated ionic clay composition. Grinding increases the surface area of the tobacco material and aids in the nicotine release and extraction process.
- the tobacco material is finely ground so that the resulting powder passes through a 5 mm mesh sieve.
- the tobacco material is finely ground so that the resulting powder passes through a 4 mm mesh sieve.
- the tobacco material is finely ground so that the resulting powder passes through a 3 mm mesh sieve.
- the tobacco material is finely ground so that the resulting powder passes through a 2 mm mesh sieve.
- the tobacco material is finely ground so that the resulting powder passes through a 1 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting power passes through a 0.5 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder has a particle size in the range of 50 microns to 2000 microns. In implementations, the tobacco material is finely ground so that the resulting powder has a particle size in the range of 100 microns to 300 microns.
- Hydrated ionic clay is mixed with a first amount of water to form a first dispersion/hydrogel, and then the powdered tobacco material is added and mixed to form a second dispersion.
- the first dispersion can have an adjusted pH value of between 5 and 12.
- the first dispersion can have a pH value of between 9 and 11.
- the first dispersion can have a pH value of between 9 and 10.
- the first amount of water can be heated, for example to a temperature of 40 °C to 80 °C.
- Mixing the hydrated ionic clay with the first amount of water can includes stirring the first dispersion until uniform.
- the second dispersion of hydrated ionic clay, water, and powdered tobacco material can be mixed until a uniform dispersion is achieved.
- a ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be greater than 1 to 1.
- a ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be greater than 2 to 1.
- a ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be from 1 to 1 to 15 to 1, including any subrange therebetween.
- a portion of the water is removed from the second dispersion. In implementations, heat is used to evaporate water from the second dispersion.
- a vacuum over is used to evaporate water from the second dispersion.
- a filter is used to remove excess water.
- a centrifuge is used to remove excess water.
- freeze drying can be used to remove excess water.
- combinations of filtering, centrifugation, and/or heating are used to remove excess water.
- FIG. 3 shows a powdered tobacco material and hydrated ionic clay composition with a portion of the water removed to form a loose cake.
- the loose cake can be compressed to form a pellet.
- the press is a hand press, a tablet press, a punch press, a stamping press, a fly press, hydraulic press, manual press, or other suitable compressive device.
- the pellet 200 is removed from the press 100.
- FIG. 4 shows a plurality of pellets 200 formed from a loose cake.
- Pellet 200 can optionally be further dried using the methods discussed above concerning drying the tobacco. Pellet 200 can optionally be humidified to achieve the desired moisture content. In implementations, pellet 200 has a moisture content of about 10 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 15 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 20 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 30 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 35 wt%.
- pellet 200 has a moisture content of about 10 wt% to about 30 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 25 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 20 wt%. In implementations, pellet 200 has a moisture content of about 15 wt% to about 35 wt%. In implementations, pellet 200 has a moisture content of about 20 wt% to about 30 wt%. In implementations, pellet 200 has a moisture content of about 5 wt% to about 10 wt%. In implementations, pellet 200 has a moisture content of less than about 10 wt%. In implementations, pellet 200 has a moisture content of about 1 wt% to about 10 wt%.
- a method of extracting nicotine from tobacco material comprises contacting tobacco material with a hydrated ionic clay to form a composition, and contacting the composition with a solvent to extract the nicotine from the tobacco material.
- the solvent can be an organic solvent.
- the solvent can be a humectant.
- the solvent can be a solution of propylene glycol and/or vegetable glycerin.
- the solvent can contain water.
- Pellet 200 is immersed in a first solution (i.e. a humectant solution) including a glycol and a glycerol.
- a first solution i.e. a humectant solution
- the first solution has a pH value of between 3 and 7.
- the first solution has a pH value of between 4 and 6.5.
- the first solution has a pH value of between 5 and 6.
- the first solution comprises a ratio of vegetable glycerin (VG) to propylene glycol (PG). The ranges of the ratio can vary between a ratio of about 100:0 VG to PG and a ratio of about 50:50 vegetable glycerol to propylene glycol.
- the ranges of the ratio can also vary between a ratio of about 50:50 vegetable glycerol to propylene glycol and a ratio of about 0: 100 VG to PG.
- the difference in preferred ratios within the above stated ranges may vary by as little as 1, for example, said ratio may be about 99:1 vegetable glycerol to propylene glycol.
- the first solution will be between the ratios of about 30:70 vegetable glycerol to propylene glycol, or about 70:30 vegetable glycerol to propylene glycol.
- the blends with varying ratios are selected for consumers with varying preferences, and based on the vaporization device.
- Water can be added to the first solution to form a second solution, which is also a humectant solution. Without being bounded to any particular theory, it is believed that water helps drive the release of nicotine from the pellet and into the solution.
- the hydrated ionic clay in water has a pH value in the range of about 8 to about 12.
- the water contacts the pellet to increase the localized pH of the hydrated ionic clay in contact with the powered tobacco material. In this manner, the nicotine in the pellet is released and extracted under a localized acidic/basic condition and then mixes into the second solution.
- the added water may also help transport the nicotine to the surface of the pellet where it can mix with the solution or a gel matrix surrounding it, the heating of which may release nicotine aerosols.
- FIG. 5A shows pellet 200 in the second solution 210 after about 0 hours.
- FIG. 5B shows pellet 200 in the second solution 210 after about 24 hours.
- the pellets 200 retain their shape in the second solution.
- the darker color of the second solution 210 in FIG. 5B indicates a high degree of extraction from the pellet 200 including higher amounts of nicotine present in the second solution 210 (also confirmed by GC-FID (Gas Chromatography/ Flame-Ionization Detection) is a good general detector for organic compounds in GC that detects the amount of carbon, however in some cases the color change may not be a direct indication of nicotine extraction).
- the second solution has a pH value of between 5 and 7.
- the second solution has a pH value of between 5 and 6.
- the second solution has a pH value of between 6 and 7.
- the second solution can be used as a vaporizable material in a vaporization device.
- flavorings can be added to the vaporizable material. These flavorings may include enhancers comprising cocoa solids, licorice, tobacco or botanical extracts, and various sugars, to name but a few.
- acids can be added to the vaporizable material. These acids may include carboxylic acids such as benzoic acid, pyruvic acid, salicylic acid, levulinic acid, malic acid, maleic acid, lactic acid, succinic acid, citric acid, and combinations thereof.
- FIG. 6 is a graph presenting the percent of nicotine extracted into the humectant with different grades of Laponite at different experimental conditions. Water and heat accelerate nicotine extraction into the humectant solution.
- FIG. 7 shows a table of pH data for multiple chemicals and compositions. While the second solution containing the humectant is acidic, the localized pH value of the tobacco material and hydrated ionic clay compositions remains basic. The tobacco material and hydrated ionic clay compositions did not make the entire solution basic. This avoids irritation in the throat while puffing as the pH did not change to basic.
- the final vaporizable material solution should be at least mildly acidic (i.e., ⁇ 7), and preferably the pH > 4.
- An example target range of the final vaporizable material solution is a pH value of about 5 to 7.
- Example 1 Method for extraction of nicotine from tobacco material-hydrated ionic clay formulation (EP) at room temperature:
- Laponite EP procured from BYK Additives Inc.
- 20 g of distilled deionized water was added to 20 g of distilled deionized water at 70 °C while constantly stirring. Once the Laponite was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure.
- 6.0 g of finely powdered tobacco material was added and mixed on high shear mixer at 2000 rpm for 5 minutes until a homogeneous dispersion of tobacco material with paste like consistency was accomplished.
- the tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration).
- Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press.
- the pellet shape could be altered to any shape or form or a powdered form could be used. Alternately, the pellet form could be directly printed using an XYZ table.
- the tobacco material-Laponite powder weighing approximately 300 mg were gently placed into a propylene glycol, vegetable glycerin, and water mixture (approximate ratio 60:30: 10) in 4.2 ml of liquid.
- the release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS.
- the nicotine released varied anywhere from 55 % to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
- Example 2 Method for extraction of nicotine from tobacco material-hydrated ionic clay formulation (RD) at room temperature:
- Laponite RD procured from BYK Additives Inc.
- 20 g of distilled deionized water was added to 20 g of distilled deionized water at 70 °C while constantly stirring. Once the Laponite was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure.
- 6.0 g of finely powdered tobacco material was added and mixed on high shear mixer at 2000 rpm for 5 minutes until a homogeneous dispersion of tobacco material with paste like consistency was accomplished.
- the tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration).
- Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press.
- the pellet shape could be altered to any shape or form or could be used in powdered form. Alternately, the pellet form could be directly printed using an XYZ table.
- the tobacco material-Laponite powder weighing approximately 300 mg were gently placed into propylene glycol, vegetable glycerin, and water mixture (approximate ratio 60:30: 10) in 4.2 ml of liquid.
- the release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS.
- the nicotine released varied anywhere from 60 % to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
- Example 3 Method for extraction of nicotine from tobacco material -hydrated ionic clay formulation (RDS) at room temperature:
- the tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration).
- Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press.
- the pellet shape could be altered to any shape or form or could be used in powdered form. Alternately, the pellet form could be directly printed using an XYZ table.
- the tobacco material-Laponite powder weighing approximately 300 mg were gently placed into Propylene Glycol, Vegetable Glycerin, and Water mixture (approximate ratio 60:30:10) in 4.2 ml of liquid.
- the release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS.
- the nicotine released varied anywhere from 60 % to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
- FIG. 7 is a graph presenting the percent of nicotine extracted for Examples 1, 2, and 3 at room temperature as described above.
- the amount of nicotine released after 6 hours was about 60 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations.
- the amount of nicotine extracted was about 80 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations.
- Example 4 Method for extrachon of nicotine from tobacco material-hydrated ionic clay formulations (EP, RD, and RDS) at elevated temperature (70 ° C):
- FIG. 8 is a graph presenting the percent of nicotine extracted for Example 4 at a temperature of 70 °C.
- the amount of nicotine released after 6 hours was about 80 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations.
- the amount of nicotine extracted was between about 75 % and 100 % by mass for each of the Laponite RD, RDS, and EP formulations.
- the amount of nicotine extracted was between about 65 % and 90 % by mass for each of the Laponite RD, RDS, and EP formulations.
- FIG. 9 is a graph presenting the percent of nicotine extracted into solution of PG/V G for several grades of Laponite at room temperature and 70 °C. Increasing the temperature tended to increase the rate of extraction for the given formulation and duration.
- Example 5 TGA-MS on Tobacco Material-Hydrated ionic clay formulations
- the formulations given in Examples 1, 2, and 3 were heated on TGA - MS (Thermogravimetric Analysis/Mass Spectrometry). All of them demonstrated nicotine release at low temperatures compared to control and competition.
- Example 6 Heating of tobacco material-hydrated ionic clay pellets (RD):
- Partially dried tobacco-Laponite gel matrix containing less than 40 % of water was compressed into a cylindrical pellet form using a 1-2 ton press.
- the pellet shape could be altered to any shape or form.
- the pellet form could be directly printed using an XYZ table.
- Wetted pellets were placed heated to 200 °C in an oven and heated for 2 minutes (without any airflow). The nicotine aerosolized was measured by what was left in pellet using GC-FID. More than 15 % nicotine release was observed after 2 minutes.
- Example 7 Heating of tobacco material-hydrated ionic clay pellets (RDS):
- Partially dried tobacco- Laponite gel matrix containing less than 40 % of water was compressed into a cylindrical pellet form using a 1-2 ton press. Pellets were wetted with humectants (approximately 80 mg ⁇ 10 % pellets and wetted with humectants). Wetted pellets were heated to 200 °C (no air flow). The nicotine aerosolized was measured by what was left in pellet using GC-FID. More than 20 % nicotine release was observed after 2 minutes.
- FIG. 10 is a graph presenting the percent of nicotine vaporized for Examples 6 and 7 at a temperature of 200 °C. Both hydrated ionic clay and tobacco material compositions released more than 2 to 2.5 times more nicotine than the tobacco control after two minutes. Terminology
- “Hydrated ionic clay” as set forth herein refers to a composition including one or more inorganic polymer layers (e.g. a clay mineral or phyllosilicate) and one or more alkali metals (e.g. sodium or magnesium) in a layered structure and is capable of forming a viscous suspension or dispersion with water.
- inorganic polymer layers e.g. a clay mineral or phyllosilicate
- alkali metals e.g. sodium or magnesium
- Water as set forth herein refers to both bound and free water within a given composition or formulation.
- references to a structure or feature that is disposed “adjacent” another feature may have portions that overlap or underlie the adjacent feature.
- Terminology used herein is for the purpose of describing particular embodiments and implementations only and is not intended to be limiting.
- the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise.
- the terms “comprises” and/or “comprising,” when used in this specification, specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof.
- the term “and/or” includes any and all combinations of one or more of the associated listed items and may be abbreviated as “/”.
- phrases such as “at least one of’ or “one or more of’ may occur followed by a conjunctive list of elements or features.
- the term “and/or” may also occur in a list of two or more elements or features. Unless otherwise implicitly or explicitly contradicted by the context in which it used, such a phrase is intended to mean any of the listed elements or features individually or any of the recited elements or features in combination with any of the other recited elements or features.
- the phrases “at least one of A and B;” “one or more of A and B;” and “A and/or B” are each intended to mean “A alone, B alone, or A and B together.”
- a similar interpretation is also intended for lists including three or more items.
- the phrases “at least one of A, B, and C;” “one or more of A, B, and C;” and “A, B, and/or C” are each intended to mean “A alone, B alone, C alone, A and B together, A and C together, B and C together, or A and B and C together.”
- Use of the term “based on,” above and in the claims is intended to mean, “based at least in part on,” such that an unrecited feature or element is also permissible.
- spatially relative terms such as “forward”, “rearward”, “under”, “below”, “lower”, “over”, “upper” and the like, may be used herein for ease of description to describe one element or feature’s relationship to another element(s) or feature(s) as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is inverted, elements described as “under” or “beneath” other elements or features would then be oriented “over” the other elements or features. Thus, the exemplary term “under” can encompass both an orientation of over and under.
- the device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
- the terms “upwardly”, “downwardly”, “vertical”, “horizontal” and the like are used herein for the purpose of explanation only unless specifically indicated otherwise.
- first and second may be used herein to describe various features/elements (including steps), these features/elements should not be limited by these terms, unless the context indicates otherwise. These terms may be used to distinguish one feature/element from another feature/element.
- a first feature/element discussed below could be termed a second feature/element
- a second feature/element discussed below could be termed a first feature/element without departing from the teachings provided herein.
- a numeric value may have a value that is +/- 0.1% of the stated value (or range of values), +/- 1% of the stated value (or range of values), +/- 2% of the stated value (or range of values), +/- 5% of the stated value (or range of values), +/- 10% of the stated value (or range of values), etc.
- Any numerical values given herein should also be understood to include about or approximately that value, unless the context indicates otherwise. For example, if the value “10” is disclosed, then “about 10” is also disclosed. Any numerical range recited herein is intended to include all sub-ranges subsumed therein.
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Abstract
Compositions made from combinations including an hydrated ionic clay and a tobacco material are described herein. Methods of manufacture, as well as methods of extracting nicotine from these compositions are also described. The compositions can be used to prepare liquid vaporizable materials by extracting nicotine from tobacco material and directly from the tobacco material and into a liquid vaporizable material.
Description
HYDRATED IONIC CLAY AND TOBACCO MATERIAL COMPOSITIONS
CROSS REFERENCE
[0001] The present application claims priority to U.S. Provisional Patent Application No. 62/951,983 entitled “Hydrated Ionic Clay and Tobacco Material Compositions” filed on December 20, 2019, which is hereby incorporated by reference in its entirety, to the extent permitted.
TECHNICAL FIELD
[0002] The subj ect matter described herein relates to compositions made from combinations that include hydrated ionic clay and plant material, such as a tobacco, and methods of extracting nicotine therefrom.
BACKGROUND
[0003] Vaporizer devices, which can also be referred to as vaporizers, electronic vaporizer devices, e-vaporizer devices or aerosolization devices, can be used for delivery of an aerosol (for example, a vapor-phase and/or condensed-phase material suspended in a stationary or moving mass of air or some other gas carrier) containing one or more active ingredients by inhalation of the aerosol by a user of the vaporizing device. For example, electronic nicotine delivery systems (ENDS) include a class of vaporizer devices that are battery powered and that can be used to simulate the experience of smoking, but without burning of tobacco or other substances. Vaporizers are gaining increasing popularity both for prescriptive medical use, in delivering medicaments, and for consumption of tobacco and other plant-based materials. Vaporizer devices can be portable, self-contained, and/or convenient for use. [0004] In use of a vaporizer device, the user inhales an aerosol, colloquially referred to as “vapor,” which can be generated by a heating element that vaporizes (e.g., causes a liquid or solid to at least partially transition to the gas phase) a vaporizable material, which can be liquid, a solution, a solid, semisolids, a paste, a wax, and/or any other form compatible for use with a specific vaporizer device. The vaporizable material used with a vaporizer can be provided within a cartridge (for example, a separable part of the vaporizer device that contains vaporizable material) that includes an outlet (for example, a mouthpiece) for vapor delivery and inhalation of the aerosol by a user.
[0005] A typical approach by which a vaporizer device generates an inhalable aerosol from a vaporizable material involves heating the vaporizable material in a vaporization chamber (or a heater chamber) to cause the vaporizable material to be converted to the gas (or vapor) phase. A vaporization chamber generally refers to an area or volume in the vaporizer device
within which a heat source (e.g., conductive, convective, and/or radiative) causes heating of a vaporizable material to produce a mixture of air and vaporized vaporizable material to form a vapor for inhalation by a user of the vaporization device.
[0006] Various vaporizable materials having a variety of contents and proportions of such contents can be contained in the cartridge. Some vaporizable materials, for example, may have a smaller percentage of active ingredients per total volume of vaporizable material, such as due to regulations requiring certain active ingredient percentages. As a result, a user may need to vaporize a large amount of vaporizable material (e.g., compared to the overall volume of vaporizable material that can be stored in a cartridge) to achieve a desired effect. [0007] In order to prepare a vaporizable material, nicotine can be extracted from tobacco or other plants and then added to a suitable carrier. One such method of extracting nicotine from tobacco is disclosed in U.S. Patent No. 2,162,738. The process disclosed therein involves extractions using ammonium hydroxide, followed by naphtha or gasoline, and a final treatment with sulfuric acid. If a portion of these harsh chemicals remained with the nicotine, it would make it unsuitable for incorporation into a vaporizable material. In addition, these extraction chemicals may not be environmentally friendly and could be difficult to dispose of after use. This extraction method may also extract undesirable compounds from the tobacco, and require extensive purification techniques to isolate the nicotine.
[0008] Assuming the nicotine is free of contaminants, it can be added to a humectant such as propylene glycol (PG), vegetable glycerin (VG), or a mixture of PG and VG (PG/V G) to form a vaporizable material. The humectant forms a solution with the nicotine and forms an aerosol after vaporization. The amount of nicotine in the vaporizable material can be adjusted by adding more or less humectant. Other additives can be incorporated into the vaporizable material such as flavorings.
SUMMARY
[0009] In certain aspects of the current subject matter, liquid vaporizable materials suitable for use in electronic vaporizer devices can be prepared by inclusion of one or more of the features described herein or comparable/equivalent approaches as would be understood by one of ordinary skill in the art. Aspects of the current subject matter relate to methods and systems extracting nicotine from tobacco or other plant material and preparing liquid vaporizable materials. In one aspect, a method of extracting nicotine from tobacco material and directly into a liquid vaporizable material is described.
[0010] In some variations, one or more of the following features may optionally be included in any feasible combination. In certain aspects of the current subject mater, a composition including a hydrated ionic clay and a tobacco material is disclosed. In certain aspects of the current subject mater, a device comprising a heating element configured to heat the composition of any one of the preceding claims to deliver nicotine or a salt thereof to a user. In certain aspects of the current subject mater, a method of extracting nicotine is disclosed. The method of extracting nicotine from tobacco material includes contacting tobacco material with hydrated ionic clay to form a composition, and contacting the composition with a solvent to extract the nicotine from the tobacco material.
[0011] In other aspects of the current subject mater, a method of extracting nicotine is disclosed. Tobacco material is ground to form powdered tobacco material. Ionic clay is mixed with a first amount of water to form a first dispersion. The powdered tobacco material is mixed with the first dispersion to form a second dispersion. A portion of the first amount of water from the second dispersion is evaporated to form a loose cake. The loose cake is compressed to form a pellet. The pellet is immersed in a first solution including a glycol and a glycerol. A second amount of water is added to the first solution to form a second solution, the second solution containing the nicotine extracted from the pellet.
[0012] In certain aspects of the current subject matter, a method of manufacturing a pellet containing tobacco material is disclosed. The method includes grinding tobacco material to form a powdered tobacco material. A hydrated ionic clay is mixed with a first amount of water to form a first dispersion. The powdered tobacco material is mixed with the first dispersion to form a second dispersion. A portion of the first amount of water is evaporated from the second dispersion to form a loose cake. The loose cake is compressed to form the pellet containing tobacco material.
[0013] In certain aspects of the subject mater, the tobacco formulation comprising hydrated ionic clays, optionally formulated with humectants such as vegetable glycerin and glycols, organic acids, flavoring agents including both natural and artificial, is subjected to temperatures in the 100 °C to 400 °C range, preferably in 150 °C to 300 °C range, to generate a vapor.
[0014] The details of one or more variations of the subject mater described herein are set forth in the accompanying drawings and the description below. Other features and advantages of the subject mater described herein will be apparent from the description and drawings, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS [0015] The accompanying drawings, which are incorporated in and constitute a part of this specification, show certain aspects of the subject matter disclosed herein and, together with the description, help explain some of the principles associated with the disclosed implementations. In the drawings:
[0016] FIG. 1 illustrates a graph of the thermal stability of hydrated ionic clays and Burley tobacco.
[0017] FIG. 2 illustrates a tobacco leaf coated with hydrated ionic clay.
[0018] FIG. 3 illustrates a tobacco powder and hydrated ionic clay composition.
[0019] FIG. 4 shows a plurality of pellets formed from powdered tobacco material and hydrated ionic clay.
[0020] FIG. 5A shows pellet in a PG/V G/water solution at 0 hours.
[0021] FIG. 5B shows pellet in a PG/V G/water solution after about 24 hours.
[0022] FIG. 6 presents a table of pH data for multiple chemicals and compositions.
[0023] FIG. 7 is a graph presenting the percent of nicotine extracted for Examples 1, 2, and 3 at room temperature.
[0024] FIG. 8 is a graph presenting the percent of nicotine extracted for Example 4 at a temperature of 70 °C.
[0025] FIG. 9 is a graph presenting the percent of nicotine extracted into solution of PG/V G for several grades of Laponite at room temperature and 70 °C.
[0026] FIG. 10 is a graph presenting the percent of nicotine vaporized for Examples 6 and 7 at a temperature of 200 °C.
[0027] When practical, similar reference numbers denote similar structures, features, or elements.
DETAILED DESCRIPTION
[0028] Implementations of the current subject matter include compositions and methods of preparing hydrated ionic clay and tobacco material compositions. The hydrated ionic clay and tobacco material compositions can be formed into a mass, such as a pellet, sheet, brick, bead, tablet, powder, semi-solid, loose cake, granulation, free flowing powder, plug, cylinder, porous rod, or other suitable shape including hollow forms with various porous structures or a coating. In other implementations, hydrated ionic clay and tobacco material compositions are in a form of a loose, powdered mixture of the hydrated ionic clay and the powdered tobacco material.
[0029] Implementations of the current subject matter also include systems and methods of extracting active ingredients (e.g. nicotine) from tobacco material and preparing vaporizable materials that may be liquid, a solution, a solid, semi-solid, loose cake, a wax, or other form as may be compatible with use of a specific vaporizer device. In implementations, the vaporizable material is a liquid comprising nicotine and a humectant that is vaporized and forms an aerosol using a vaporizer. Vaporizer is used generically in the following description to refer to a vaporizer device. Examples of vaporizers consistent with implementations of the current subject matter include electronic vaporizers, combustible vaporizers, or the like. Such vaporizers are generally portable, hand-held devices that heat a vaporizable material to provide an inhalable dose of the vaporizable material.
[0030] The vaporizable material used with a vaporizer may optionally be provided within a cartridge (e.g., a part of the vaporizer that contains the vaporizable material in a reservoir or other container and that can be refillable when empty or disposable in favor of a new cartridge containing additional vaporizable material of a same or different type). A vaporizer may be a cartridge-using vaporizer, a cartridge-less vaporizer, or a multi-use vaporizer capable of use with or without a cartridge. For example, a multi-use vaporizer may include a heating chamber (e.g., an oven) configured to receive a vaporizable material directly in the heating chamber and also to receive a cartridge or other replaceable device having a reservoir, a volume, or the like for at least partially containing a usable amount of vaporizable material.
[0031] In various implementations, a liquid vaporizable material (e.g., a carrier solution in which an active and/or inactive ingredient(s) are suspended or held in solution or a neat liquid form of the vaporizable material itself) can be prepared. A liquid vaporizable material can likewise be capable of being completely vaporized or can include some part of the liquid material that remains after all of the material suitable for inhalation has been consumed. [0032] In various implementations, nicotine is extracted from tobacco material into a humectant. In other words, nicotine is extracted directly from tobacco material (e.g. powdered tobacco within the hydrated ionic clay and tobacco composition), and into solution with a humectant such as a PG/VG mixture. In this manner, the nicotine extraction process avoids the need for a separate extraction process to obtain the nicotine, which would in turn be added into a humectant. Natural extraction of nicotine, alkaloids, and flavoring agents directly into PG/VG may eliminate the need for formulating an e-liquid with synthetic nicotine and flavoring agents. Additional flavors or additives to customize the extractant formulation can be added, if required. Implementations according to the present
process also avoid the need for subsequent purification of a tobacco material extract to obtain the nicotine, which may be required step for other extraction processes. Implementations according to the present process also avoid the use of harsh or toxic chemicals that can contaminate the nicotine and ultimately the vaporizable material. Implementations according to the present process also avoid the need for high temperature extraction processes, or high temperature purification processes, since the nicotine can be extracted from the tobacco material at standard conditions (i.e. room temperature, standard pressure). Without being bounded to any particular theory, it is believed that implementations according to the present process selectively extract nicotine/alkaloids from a tobacco material while avoiding the extraction of undesirable, higher molecular weight compounds, as compared to other extraction processes.
[0033] Various implementations include the release of nicotine at lower temperatures into a vapor form. Various implementations include permeating water into a tobacco structure for migration of nicotine/alkaloids. Various implementations include release of nicotine in final product in the pH range of 5 to 8. Various implementations include release of nicotine from tobacco into a gel matrix. Various implementations include release of nicotine into viscous liquids or semi solids or hydrogels. Various implementations include pre-heating of the product to improve nicotine release efficiency at low temperatures. Various implementations include use of clays as binders to modify the bulk density, rod density, porosity, flow properties, compressibility, thermal conductivity, form factors, moldability, processability, and manufacturability of a composition. Various implementations include compositions comprising a thermally stable clay and like materials, which optionally do not release any organic materials below 300 °C. Various implementations enable multiple heating element designs and form factors to make it compact and energy efficient. Various implementations include wetting agents or humectants along with ionic clays.
[0034] Implementations according to the present disclosure are suitable for industrial scale extraction of nicotine from tobacco material. Implementations according to the present disclosure are suitable for in situ extraction of nicotine from tobacco material within a personal-sized, vaporization device.
[0035] In order to facilitate the release or extraction of nicotine from the tobacco material, a hydrated ionic clay is added to the tobacco material. Without being bounded to any particular theory, it is believed that the hydrated ionic clay in the hydrated ionic clay and tobacco material composition facilitates an nicotine exchange process that allows nicotine to be released from the tobacco material. In this manner, nicotine is released from the
tobacco material and migrates to a surface of a tobacco material/hydrated ionic clay matrix. The nicotine may be stabilized on the surface of the matrix by hydrogen bonding and/or ionic bonding. Alternately, without bound by the theory, it is possible that tobacco/hydrated ionic clay create acid/base junction in solid phase or pH gradient, and it is possible that the presence of polar solvents such as water could transport nicotine to the intersection of tobacco/ hydrated ionic clay from the interior of tobacco. From the surface of the matrix, the nicotine can be extracted into a humectants to form e-liquids, or heated (optionally in presence of humectants) to form an aerosol containing nicotine. The nicotine transport process occurs within the tobacco material/hydrated ionic clay matrix. Also under the basic conditions, bound nicotine is converted to free base nicotine. However, it is understood that protonated and freebase nicotine may exist in equilibrium, and that the composition of each formed inside tobacco is governed by the localized pH. When extracted from the tobacco, the equilibrium of protonated and freebase nicotine dynamically change or switch based on environmental conditions of the tobacco material/hydrated ionic clay matrix and temperature. Increasing the temperature increases the rate of nicotine release from tobacco material/hydrated ionic clay matrix, as well as increasing the rate of extraction of the nicotine into the humectant. The addition of water can facilitate the nicotine/ion exchange process and release of nicotine to the surface of the matrix. The addition of water can also facilitate the release of nicotine from the tobacco material at lower temperatures as compared to the absence of added water. However, the mobility of the nicotine release may be impacted by structured water versus free water differently.
[0036] In implementations, the composition comprises a hydrated ionic clay and a tobacco material. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 4 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 2 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay in an amount between 0.1 wt% to 5 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay in an amount between 0.1 wt% to 10 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 40 wt% to 99 wt% of the composition, and any subranges therebetween. The composition can comprise
the tobacco material in an amount between 40 wt% to 90 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 40 wt% to 80 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 40 wt% to 70 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 40 wt% to 60 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 40 wt% to 50 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 50 wt% to 90 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 50 wt% to 80 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 50 wt% to 70 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 50 wt% to 60 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 80 wt% to 99 wt% of the composition, and any subranges therebetween. The composition can comprise the tobacco material in an amount between 90 wt% to 99 wt% of the composition, and any subranges therebetween. In implementations, the composition further comprises water. The composition can comprise the water in an amount between 5 wt% to 50 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 5 wt% to 40 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 5 wt% to 30 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 5 wt% to 20 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 5 wt% to 15 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 10 wt% to 40 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 10 wt% to 30 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 10 wt% to 20 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 10 wt% to 15 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 1 wt% to 10 wt% of the composition, and any subranges therebetween. The
composition can comprise the water in an amount between 1 wt% to 5 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 0.1 wt% to 10 wt% of the composition, and any subranges therebetween. The composition can comprise the water in an amount between 2 wt% to 6 wt% of the composition, and any subranges therebetween. The composition can comprise the hydrated ionic clay and the tobacco material in any of the aforementioned amounts, except in combinations where such amounts are mutually exclusive. The composition can comprise the hydrated ionic clay, the tobacco material, and water in any of the aforementioned amounts, except in combinations where such amounts are mutually exclusive.
[0037] In implementations, the composition comprises a hydrated ionic clay, a tobacco material, and water. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 5 wt%, the tobacco material in an amount between 40 wt% to 99 wt%, and the water in an amount between 5 wt% to 50 wt% of the composition. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 4 wt%, the tobacco material in an amount between 50 wt% to 90 wt%, and the water in an amount between 5 wt% to 40 wt% of the composition. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 3 wt%, the tobacco material in an amount between 60 wt% to 90 wt%, and the water in an amount between 5 wt% to 30 wt% of the composition. The composition can comprise the hydrated ionic clay in an amount between 1 wt% to 3 wt%, the tobacco material in an amount between 50 wt% to 90 wt%, and the water in an amount between 10 wt% to 30 wt% of the composition.
[0038] In implementations, the hydrated ionic clay is a synthetic layered material carrying either a negative charge or a positive charge. The hydrated ionic clay can be an anionic layered alkaline clay. The hydrated ionic clay can comprise silicates. The hydrated ionic clay can comprise alkali and/or alkaline earth metal silicates. The hydrated ionic clay can be a magnesium silicate clay. The hydrated ionic clay can be a sodium magnesium silicate clay. The hydrated ionic clay can be a synthetic trioctahedral clay mineral. The hydrated ionic clay comprises aluminates, titanates and/or zirconates. The hydrated ionic clay can be an aluminate, such as layered double hydroxide carrying net positive charge. The hydrated ionic clay can be a synthetic phyllosilicate. The synthetic phyllosilicate can be a lithium magnesium sodium orthosilicate. The hydrated ionic clay can comprise phosphates. The synthetic phyllosilicate can be an inorganic composition comprising hydrogen, lithium, magnesium, sodium, oxygen, and silicon. The inorganic composition is dilithium;hexadecamagnesium;disodium;l,3,5,7-tetraoxido-2,4,6,8,9,10-hexaoxa-l,3,5,7-
tetrasilatricyclo[3.3.1.13,7]decane;dodecahydroxide. The hydrated ionic clay can include an additive within the clay matrix. The hydrated ionic clay can be Laponite. Laponite, also known as hectorite, is a synthetic, colloidal, layered silicate manufactured from naturally occurring minerals. Laponite, an inorganic polymer, has higher gelling strength and can hold more tobacco material than natural clays. Laponite is available in multiple different grades. The hydrated ionic clay is a gel forming grade, e.g. a gel forming grade of Laponite. The hydrated ionic clay is a gel forming grade, e.g. a sol forming grade of Laponite.
[0039] Water can be added to the ionic clay to form a hydrated ionic clay. A portion of the water in the hydrated ionic clay can be bound within the crystalline lattice, with any excess water being free moisture. The hydrated ionic clay may have a surface hydroxyl concentration contributing to localized negative charges. Other moieties including silicon oxides may also contribute to the hydrated ionic clay’s anionic properties. Mg2+, Li+, K+, and Na+ ions may contribute to a localized positive charges, and also serve as exchangeable cations for the hydrated ionic clay. The charged nature and the interlayer space within the hydrated ionic clay can provide for adsorption of organic molecules.
[0040] In implementations, the tobacco material includes one or more types of tobacco. The tobacco material can be a single type of tobacco or a blend. Any variety of tobacco can be used including, but not limited to, Aromatic Fire-cured, Brightleaf, Burley, Cavendish, Corojo, Criollo, Dokha, Ecuadorian Sumatra, Habano, Kasturi, Latakia, Maduro, Oriental, Perique, Shade, Thuoc lao, Type 22, Virginia, White Burley, Wild, Yl, and the like. The tobacco material may be dry-ice expanded tobacco (DIET), Hue-cured tobacco, and/or air- cured tobacco.
[0041] In implementations, the composition is contained within a cartridge. In implementations, the composition is heated in a device comprising a heating element configured to heat the composition to deliver nicotine or a salt thereof to a user. The device can be an electronic nicotine delivery system.
[0042] FIG. 1 shows a graph of the thermal stability of two grades of Laponite and Burley tobacco material. The initial weight loss at 100 °C of the Laponite is attributable to the loss of the free water. In all, the Laponite loses less than about 10% of its weight up to 600 °C, with almost all of the weight loss being water. On the other hand, tobacco loses 60 % of its weight before reaching 400 °C. Hydrated ionic clays, such as Laponite, are non-flammable and thermally stable at temperatures below 800 °C.
[0043] In implementations, the hydrated ionic clay (e.g. Laponite) is gel forming grade the forms a high viscosity colloidal dispersion with water. In implementations, the hydrated
ionic clay is sol forming grade the forms a low viscosity colloidal dispersion with water. While the actual viscosity of the colloidal dispersion depends on the amount of hydrated ionic clay used in the dispersion, the aforementioned high and low viscosity descriptors refer to relative viscosities at a given concentration.
[0044] Laponite forms an alkaline dispersion that has a basic pH value, with many of the dispersions having a pH value between 9 and 10. It is believed that all grades of Laponite that have a basic pH can be used in the formulation. However, Laponites could be stabilized to neutral or lower pH by adding acids, for example, to create dispersions having a final pH value of the range from 5 to 12. The acids can be organic acids such as carboxylic acids or inorganic acids such as phosphoric acid.
[0045] In implementations, the tobacco leaves are dried or cured to remove excess moisture and break down chemical compounds. Methods of drying or curing tobacco material include air drying, oven drying, flame-curing, convective drying, vacuum drying, free drying, and combinations thereof. Any type of tobacco material is generally suitable for use according the methods and systems disclosed herein. In implementations, the tobacco material is a Burley tobacco.
[0046] Before use, the hydrated ionic clay is hydrated. For example, a quantity of hydrated ionic clay is measured and added to warm water. The water may be heated to a temperature of 40 °C to 80 °C. Heating the water helps the rate at which the hydrated ionic clay disperses in the water. The composition can be mixed by stirring until a uniform dispersion is achieved.
[0047] In implementations, whole tobacco leaves are coated with hydrated ionic clay as shown in FIG. 2. Coating the whole tobacco leaf can be completed before or after the aforementioned drying process. The hydrated ionic clay coating can be applied by a spraying process, contact process (e.g. brushing) or by dipping the leaf in a hydrated ionic clay dispersion. Coating the tobacco leaf with hydrated ionic clay prior to a drying or curing process can avoid multiple drying steps and facilitate the breakdown of chemical compounds. Coating the whole tobacco leaf with hydrated ionic clay can also be accomplished a minimal need for capital investment in equipment. After coating with the hydrated ionic clay, the tobacco leaf can be rolled, cut, pulverized, and/or ground into a powder.
[0048] In implementations, a method of manufacturing a pellet (or other compressed form) containing tobacco material comprises grinding tobacco material to form a powdered tobacco (particle size distribution may range from 50 to 5000 microns) material, mixing a
hydrated ionic clay with a first amount of water to form a first dispersion, mixing the powdered tobacco material with the first dispersion to form a second dispersion, evaporating a portion of the first amount of water from the second dispersion to form a loose cake, and compressing the loose cake to form the pellet containing tobacco material. In an initial step, the tobacco leaves are ground to form a powdered tobacco material. In implementations, the tobacco leaves coated with hydrated ionic clay are ground to form a powdered tobacco material and hydrated ionic clay composition. Grinding increases the surface area of the tobacco material and aids in the nicotine release and extraction process. In implementations, the tobacco material is finely ground so that the resulting powder passes through a 5 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder passes through a 4 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder passes through a 3 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder passes through a 2 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder passes through a 1 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting power passes through a 0.5 mm mesh sieve. In implementations, the tobacco material is finely ground so that the resulting powder has a particle size in the range of 50 microns to 2000 microns. In implementations, the tobacco material is finely ground so that the resulting powder has a particle size in the range of 100 microns to 300 microns.
[0049] Hydrated ionic clay is mixed with a first amount of water to form a first dispersion/hydrogel, and then the powdered tobacco material is added and mixed to form a second dispersion. The first dispersion can have an adjusted pH value of between 5 and 12. The first dispersion can have a pH value of between 9 and 11. The first dispersion can have a pH value of between 9 and 10. The first amount of water can be heated, for example to a temperature of 40 °C to 80 °C. Mixing the hydrated ionic clay with the first amount of water can includes stirring the first dispersion until uniform.
[0050] The second dispersion of hydrated ionic clay, water, and powdered tobacco material can be mixed until a uniform dispersion is achieved. A ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be greater than 1 to 1. A ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be greater than 2 to 1. A ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion can be from 1 to 1 to 15 to 1, including any subrange therebetween.
[0051] After mixing, a portion of the water is removed from the second dispersion. In implementations, heat is used to evaporate water from the second dispersion. In implementations, a vacuum over is used to evaporate water from the second dispersion. In implementations, a filter is used to remove excess water. In implementations, a centrifuge is used to remove excess water. In implementations, freeze drying can be used to remove excess water. In implementations, combinations of filtering, centrifugation, and/or heating are used to remove excess water.
[0052] After removing a portion of the excess water, a loose cake is formed. FIG. 3 shows a powdered tobacco material and hydrated ionic clay composition with a portion of the water removed to form a loose cake. The loose cake can be compressed to form a pellet. In implementations, the press is a hand press, a tablet press, a punch press, a stamping press, a fly press, hydraulic press, manual press, or other suitable compressive device. After pressing, the pellet 200 is removed from the press 100. FIG. 4 shows a plurality of pellets 200 formed from a loose cake.
[0053] Pellet 200 can optionally be further dried using the methods discussed above concerning drying the tobacco. Pellet 200 can optionally be humidified to achieve the desired moisture content. In implementations, pellet 200 has a moisture content of about 10 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 15 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 20 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 30 wt% to about 40 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 35 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 30 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 25 wt%. In implementations, pellet 200 has a moisture content of about 10 wt% to about 20 wt%. In implementations, pellet 200 has a moisture content of about 15 wt% to about 35 wt%. In implementations, pellet 200 has a moisture content of about 20 wt% to about 30 wt%. In implementations, pellet 200 has a moisture content of about 5 wt% to about 10 wt%. In implementations, pellet 200 has a moisture content of less than about 10 wt%. In implementations, pellet 200 has a moisture content of about 1 wt% to about 10 wt%.
[0054] In implementations, a method of extracting nicotine from tobacco material comprises contacting tobacco material with a hydrated ionic clay to form a composition, and contacting the composition with a solvent to extract the nicotine from the tobacco material. The solvent can be an organic solvent. The solvent can be a humectant. For
example, the solvent can be a solution of propylene glycol and/or vegetable glycerin. The solvent can contain water.
[0055] Pellet 200 is immersed in a first solution (i.e. a humectant solution) including a glycol and a glycerol. In implementations, the first solution has a pH value of between 3 and 7. In implementations, the first solution has a pH value of between 4 and 6.5. In implementations, the first solution has a pH value of between 5 and 6. In implementations, the first solution comprises a ratio of vegetable glycerin (VG) to propylene glycol (PG). The ranges of the ratio can vary between a ratio of about 100:0 VG to PG and a ratio of about 50:50 vegetable glycerol to propylene glycol. The ranges of the ratio can also vary between a ratio of about 50:50 vegetable glycerol to propylene glycol and a ratio of about 0: 100 VG to PG. The difference in preferred ratios within the above stated ranges may vary by as little as 1, for example, said ratio may be about 99:1 vegetable glycerol to propylene glycol. However, more commonly said ratios would vary in increments of 15, for example, about 95:5 vegetable glycerol to propylene glycol; or about 85:15 vegetable glycerol to propylene glycol; or about 70:30 vegetable glycerol to propylene glycol; or about 55:45 vegetable glycerol to propylene glycol; or about 40:60 vegetable glycerol to propylene glycol; or about 25:75 vegetable glycerol to propylene glycol; or about 10:90 vegetable glycerol to propylene glycol. In preferred implementations, the first solution will be between the ratios of about 30:70 vegetable glycerol to propylene glycol, or about 70:30 vegetable glycerol to propylene glycol. The blends with varying ratios are selected for consumers with varying preferences, and based on the vaporization device.
[0056] Water can be added to the first solution to form a second solution, which is also a humectant solution. Without being bounded to any particular theory, it is believed that water helps drive the release of nicotine from the pellet and into the solution. The hydrated ionic clay in water has a pH value in the range of about 8 to about 12. By adding a small amount of water to the second solution containing the pellet, the water contacts the pellet to increase the localized pH of the hydrated ionic clay in contact with the powered tobacco material. In this manner, the nicotine in the pellet is released and extracted under a localized acidic/basic condition and then mixes into the second solution. The added water may also help transport the nicotine to the surface of the pellet where it can mix with the solution or a gel matrix surrounding it, the heating of which may release nicotine aerosols.
[0057] FIG. 5A shows pellet 200 in the second solution 210 after about 0 hours. FIG. 5B shows pellet 200 in the second solution 210 after about 24 hours. The pellets 200 retain their shape in the second solution. The darker color of the second solution 210 in FIG. 5B
indicates a high degree of extraction from the pellet 200 including higher amounts of nicotine present in the second solution 210 (also confirmed by GC-FID (Gas Chromatography/ Flame-Ionization Detection) is a good general detector for organic compounds in GC that detects the amount of carbon, however in some cases the color change may not be a direct indication of nicotine extraction). In implementations, the second solution has a pH value of between 5 and 7. In implementations, the second solution has a pH value of between 5 and 6. In implementations, the second solution has a pH value of between 6 and 7.
[0058] After a desired amount of nicotine is extracted from the pellet, the second solution can be used as a vaporizable material in a vaporization device. In implementations, flavorings can be added to the vaporizable material. These flavorings may include enhancers comprising cocoa solids, licorice, tobacco or botanical extracts, and various sugars, to name but a few. In implementations, acids can be added to the vaporizable material. These acids may include carboxylic acids such as benzoic acid, pyruvic acid, salicylic acid, levulinic acid, malic acid, maleic acid, lactic acid, succinic acid, citric acid, and combinations thereof.
[0059] FIG. 6 is a graph presenting the percent of nicotine extracted into the humectant with different grades of Laponite at different experimental conditions. Water and heat accelerate nicotine extraction into the humectant solution.
[0060] FIG. 7 shows a table of pH data for multiple chemicals and compositions. While the second solution containing the humectant is acidic, the localized pH value of the tobacco material and hydrated ionic clay compositions remains basic. The tobacco material and hydrated ionic clay compositions did not make the entire solution basic. This avoids irritation in the throat while puffing as the pH did not change to basic. The final vaporizable material solution should be at least mildly acidic (i.e., < 7), and preferably the pH > 4. An example target range of the final vaporizable material solution is a pH value of about 5 to 7.
[0061] Example 1. Method for extraction of nicotine from tobacco material-hydrated ionic clay formulation (EP) at room temperature:
[0062] Approximately 0.4 g of Laponite EP (procured from BYK Additives Inc.) was added to 20 g of distilled deionized water at 70 °C while constantly stirring. Once the Laponite was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure. To 20.4 g of the sol/gel, 6.0 g of finely powdered tobacco material (Burley, particle size ranging from 100-500 microns), was added and
mixed on high shear mixer at 2000 rpm for 5 minutes until a homogeneous dispersion of tobacco material with paste like consistency was accomplished. The tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration). Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press. However, the pellet shape could be altered to any shape or form or a powdered form could be used. Alternately, the pellet form could be directly printed using an XYZ table. The tobacco material-Laponite powder weighing approximately 300 mg were gently placed into a propylene glycol, vegetable glycerin, and water mixture (approximate ratio 60:30: 10) in 4.2 ml of liquid. The release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS. The nicotine released varied anywhere from 55 % to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
[0063] Example 2. Method for extraction of nicotine from tobacco material-hydrated ionic clay formulation (RD) at room temperature:
[0064] Approximately 0.4 g of Laponite RD (procured from BYK Additives Inc.) was added to 20 g of distilled deionized water at 70 °C while constantly stirring. Once the Laponite was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure. To 20.4 g of the sol/gel, 6.0 g of finely powdered tobacco material (Burley, particle size ranging from 100-500 microns), was added and mixed on high shear mixer at 2000 rpm for 5 minutes until a homogeneous dispersion of tobacco material with paste like consistency was accomplished. The tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration). Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press. However, the pellet shape could be altered to any shape or form or could be used in powdered form. Alternately, the pellet form could be directly printed using an XYZ table. The tobacco material-Laponite powder weighing approximately 300 mg were gently placed into propylene glycol, vegetable glycerin, and water mixture (approximate ratio 60:30: 10) in 4.2 ml of liquid. The release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS. The nicotine released varied anywhere from 60
% to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
[0065] Example 3. Method for extraction of nicotine from tobacco material -hydrated ionic clay formulation (RDS) at room temperature:
[0066] Approximately 0.4 g of Laponite RDS (procured from BYK Additives Inc.) was added to 20 g of distilled deionized water at 70 °C while constantly stirring. Once the Laponite was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure. To 20.4 g of the sol/gel, 6.0 g of finely powdered tobacco material (Burley, particle size ranging from 100-500 microns), was added and mixed on high shear mixer at 2000 rpm for 5 minutes until a homogeneous dispersion of tobacco material with paste like consistency was accomplished. The tobacco material particles suspended in gel structure were partially dehydrated (optionally) until the final concentration of the water in the formulation is less than 40% (as determined by Karl Fischer titration). Partially dried tobacco material-Laponite gel matrix containing less than 40% of water was compressed into a cylindrical pellet form using a 1-2 ton press. However, the pellet shape could be altered to any shape or form or could be used in powdered form. Alternately, the pellet form could be directly printed using an XYZ table. The tobacco material-Laponite powder weighing approximately 300 mg were gently placed into Propylene Glycol, Vegetable Glycerin, and Water mixture (approximate ratio 60:30:10) in 4.2 ml of liquid. The release of nicotine from the from tobacco Laponite mixture at room temperature was measured using LC-MS. The nicotine released varied anywhere from 60 % to 80 % by mass based on experimental conditions employed (i.e., time, temperature and solvent ratios).
[0067] FIG. 7 is a graph presenting the percent of nicotine extracted for Examples 1, 2, and 3 at room temperature as described above. The amount of nicotine released after 6 hours was about 60 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations. After 24 hours, the amount of nicotine extracted was about 80 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations. After 48 hours extraction, there were minimal changes for each of the three Laponite grades.
[0068] Example 4. Method for extrachon of nicotine from tobacco material-hydrated ionic clay formulations (EP, RD, and RDS) at elevated temperature (70 °C):
[0069] All the tobacco clay formulations given in Examples 1, 2, and 3 were extracted into same solvents (as in given Examples 1, 2, and 3) at 70 °C to study the effect of temperature on nicotine release. FIG. 8 is a graph presenting the percent of nicotine extracted for
Example 4 at a temperature of 70 °C. The amount of nicotine released after 6 hours was about 80 % + 5 % by mass for each of the Laponite RD, RDS, and EP formulations. After 24 hours, the amount of nicotine extracted was between about 75 % and 100 % by mass for each of the Laponite RD, RDS, and EP formulations. After 48 hours extraction the amount of nicotine extracted was between about 65 % and 90 % by mass for each of the Laponite RD, RDS, and EP formulations.
[0070] The results of all the extraction studies at both room temperature and 70 °C are summarized in Table 1, below.
[0071] FIG. 9 is a graph presenting the percent of nicotine extracted into solution of PG/V G for several grades of Laponite at room temperature and 70 °C. Increasing the temperature tended to increase the rate of extraction for the given formulation and duration.
[0072] Example 5. TGA-MS on Tobacco Material-Hydrated ionic clay formulations [0073] The formulations given in Examples 1, 2, and 3 were heated on TGA - MS (Thermogravimetric Analysis/Mass Spectrometry). All of them demonstrated nicotine release at low temperatures compared to control and competition.
[0074] Example 6. Heating of tobacco material-hydrated ionic clay pellets (RD):
[0075] Approximately 0.4 g of Laponite RD (procured from BYK Additives Inc.) was added to 20 g of distilled deionized water at 60 °C while constantly stirring. Once Laponite RD was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure. To 20.4 g sol/gel, 6.0 g of finely powdered Tobacco (Burley, particle size ranges from 100-500 microns), was added and rigorously agitated until a homogeneous dispersion of tobacco with paste like consistency is accomplished. The tobacco particles suspended in tobacco were partially dehydrated until the final concentration of the water in the formulation is less than 40 % (as determined by Karl
Fisher). Partially dried tobacco-Laponite gel matrix containing less than 40 % of water was compressed into a cylindrical pellet form using a 1-2 ton press. However, the pellet shape could be altered to any shape or form. Alternately, the pellet form could be directly printed using an XYZ table. Weighed approximately 80 mg ± 10 % pellets and wetted with humectants. Wetted pellets were placed heated to 200 °C in an oven and heated for 2 minutes (without any airflow). The nicotine aerosolized was measured by what was left in pellet using GC-FID. More than 15 % nicotine release was observed after 2 minutes.
[0076] Example 7. Heating of tobacco material-hydrated ionic clay pellets (RDS):
[0077] Approximately 0.4 g of Laponite RDS (procured from BYK Additives Inc.) was added to 20 g of distilled deionized water at 60 °C while constantly stirring. Once Laponite RDS was fully dissolved or dispersed, the viscosity of the water significantly increased and eventually formed a sol/gel structure. To 20.4 g sol/gel, 6.0 g of finely powdered Tobacco (Burley, particle size 100-500 microns), was added and rigorously agitated until a homogeneous dispersion of tobacco with paste like consistency is accomplished. The tobacco pellet was partially dehydrated until the final concentration of the water in the formulation is less than 40 % (as determined by Karl Fisher). Partially dried tobacco- Laponite gel matrix containing less than 40 % of water was compressed into a cylindrical pellet form using a 1-2 ton press. Pellets were wetted with humectants (approximately 80 mg ± 10 % pellets and wetted with humectants). Wetted pellets were heated to 200 °C (no air flow). The nicotine aerosolized was measured by what was left in pellet using GC-FID. More than 20 % nicotine release was observed after 2 minutes.
[0078] FIG. 10 is a graph presenting the percent of nicotine vaporized for Examples 6 and 7 at a temperature of 200 °C. Both hydrated ionic clay and tobacco material compositions released more than 2 to 2.5 times more nicotine than the tobacco control after two minutes. Terminology
[0079] “Hydrated ionic clay” as set forth herein refers to a composition including one or more inorganic polymer layers (e.g. a clay mineral or phyllosilicate) and one or more alkali metals (e.g. sodium or magnesium) in a layered structure and is capable of forming a viscous suspension or dispersion with water.
[0080] “Water” as set forth herein refers to both bound and free water within a given composition or formulation.
[0081] When a feature or element is herein referred to as being “on” another feature or element, it can be directly on the other feature or element or intervening features and/or elements may also be present. In contrast, when a feature or element is referred to as being
“directly on” another feature or element, there are no intervening features or elements present. It will also be understood that, when a feature or element is referred to as being “connected”, “attached” or “coupled” to another feature or element, it can be directly connected, attached or coupled to the other feature or element or intervening features or elements may be present. In contrast, when a feature or element is referred to as being “directly connected”, “directly attached” or “directly coupled” to another feature or element, there are no intervening features or elements present.
[0082] Although described or shown with respect to one embodiment, the features and elements so described or shown can apply to other embodiments. It will also be appreciated by those of skill in the art that references to a structure or feature that is disposed “adjacent” another feature may have portions that overlap or underlie the adjacent feature.
[0083] Terminology used herein is for the purpose of describing particular embodiments and implementations only and is not intended to be limiting. For example, as used herein, the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises” and/or “comprising,” when used in this specification, specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof. As used herein, the term “and/or” includes any and all combinations of one or more of the associated listed items and may be abbreviated as “/”.
[0084] In the descriptions above and in the claims, phrases such as “at least one of’ or “one or more of’ may occur followed by a conjunctive list of elements or features. The term “and/or” may also occur in a list of two or more elements or features. Unless otherwise implicitly or explicitly contradicted by the context in which it used, such a phrase is intended to mean any of the listed elements or features individually or any of the recited elements or features in combination with any of the other recited elements or features. For example, the phrases “at least one of A and B;” “one or more of A and B;” and “A and/or B” are each intended to mean “A alone, B alone, or A and B together.” A similar interpretation is also intended for lists including three or more items. For example, the phrases “at least one of A, B, and C;” “one or more of A, B, and C;” and “A, B, and/or C” are each intended to mean “A alone, B alone, C alone, A and B together, A and C together, B and C together, or A and B and C together.” Use of the term “based on,” above and in the claims is intended to mean, “based at least in part on,” such that an unrecited feature or element is also permissible.
[0085] Spatially relative terms, such as “forward”, “rearward”, “under”, “below”, “lower”, “over”, “upper” and the like, may be used herein for ease of description to describe one element or feature’s relationship to another element(s) or feature(s) as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is inverted, elements described as “under” or “beneath” other elements or features would then be oriented “over” the other elements or features. Thus, the exemplary term “under” can encompass both an orientation of over and under. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly. Similarly, the terms “upwardly”, “downwardly”, “vertical”, “horizontal” and the like are used herein for the purpose of explanation only unless specifically indicated otherwise. [0086] Although the terms “first” and “second” may be used herein to describe various features/elements (including steps), these features/elements should not be limited by these terms, unless the context indicates otherwise. These terms may be used to distinguish one feature/element from another feature/element. Thus, a first feature/element discussed below could be termed a second feature/element, and similarly, a second feature/element discussed below could be termed a first feature/element without departing from the teachings provided herein.
[0087] As used herein in the specification and claims, including as used in the examples and unless otherwise expressly specified, all numbers may be read as if prefaced by the word “about” or “approximately,” even if the term does not expressly appear. The phrase “about” or “approximately” may be used when describing magnitude and/or position to indicate that the value and/or position described is within a reasonable expected range of values and/or positions. For example, a numeric value may have a value that is +/- 0.1% of the stated value (or range of values), +/- 1% of the stated value (or range of values), +/- 2% of the stated value (or range of values), +/- 5% of the stated value (or range of values), +/- 10% of the stated value (or range of values), etc. Any numerical values given herein should also be understood to include about or approximately that value, unless the context indicates otherwise. For example, if the value “10” is disclosed, then “about 10” is also disclosed. Any numerical range recited herein is intended to include all sub-ranges subsumed therein. It is also understood that when a value is disclosed that “less than or equal to” the value, “greater than or equal to the value” and possible ranges between values are also disclosed, as appropriately understood by the skilled artisan. For example, if the value “X” is disclosed
the “less than or equal to X” as well as “greater than or equal to X” (e.g., where X is a numerical value) is also disclosed. It is also understood that the throughout the application, data is provided in a number of different formats, and that this data, represents endpoints and starting points, and ranges for any combination of the data points. For example, if a particular data point “10” and a particular data point “15” are disclosed, it is understood that greater than, greater than or equal to, less than, less than or equal to, and equal to 10 and 15 are considered disclosed as well as between 10 and 15. It is also understood that each unit between two particular units are also disclosed. For example, if 10 and 15 are disclosed, then 11, 12, 13, and 14 are also disclosed.
[0088] As used herein in the specification and claims, all ratios are determined on a mass/mass basis.
[0089] Although various illustrative embodiments are described above, any of a number of changes may be made to various embodiments without departing from the teachings herein. For example, the order in which various described method steps are performed may often be changed in alternative embodiments, and in other alternative embodiments, one or more method steps may be skipped altogether. Optional features of various device and system embodiments may be included in some embodiments and not in others. Therefore, the foregoing description is provided primarily for exemplary purposes and should not be interpreted to limit the scope of the claims.
[0090] The examples and illustrations included herein show, by way of illustration and not of limitation, specific embodiments in which the subject matter may be practiced. As mentioned, other embodiments may be utilized and derived there from, such that structural and logical substitutions and changes may be made without departing from the scope of this disclosure. Such embodiments of the inventive subject matter may be referred to herein individually or collectively by the term “invention” merely for convenience and without intending to voluntarily limit the scope of this application to any single invention or inventive concept, if more than one is, in fact, disclosed. Thus, although specific embodiments have been illustrated and described herein, any arrangement calculated to achieve the same purpose may be substituted for the specific embodiments shown. This disclosure is intended to cover any and all adaptations or variations of various embodiments. Combinations of the above embodiments, and other embodiments not specifically described herein, will be apparent to those of skill in the art upon reviewing the above description.
Claims
1. A composition comprising: a hydrated ionic clay and a tobacco material.
2. The composition of claim 1, wherein the hydrated ionic clay is between 1 wt% to 10 wt% of the composition.
3. The composition of claim 2, wherein the hydrated ionic clay is between 1 wt% to 4 wt% of the composition.
4. The composition of claim 3, wherein the hydrated ionic clay is between 1 wt% to 3 wt% of the composition.
5. The composition of claim 4, wherein the hydrated ionic clay is between 1 wt% to 2 wt% of the composition.
6. The composition of any one of the preceding claims, wherein the tobacco material is between 20 wt% to 95 wt% of the composition.
7. The composition of claim 6, wherein the tobacco material is between 40 wt% to 90 wt% of the composition.
8. The composition of claim 7, wherein the tobacco material is between 40 wt% to 80 wt% of the composition.
9. The composition of claim 8, wherein the tobacco material is between 40 wt% to 60 wt% of the composition.
10. The composition of claim 9, wherein the tobacco material is between 40 wt% to 50 wt% of the composition.
11. The composition of claim 6, wherein the tobacco material is between 50 wt% to 90 wt% of the composition.
12. The composition of claim 11, wherein the tobacco material is between 50 wt% to 80 wt% of the composition.
13. The composition of claim 12, wherein the tobacco material is between 50 wt% to 70 wt% of the composition.
14. The composition of claim 13, wherein the tobacco material is between 50 wt% to 60 wt% of the composition.
15. The composition of claim 6, wherein the tobacco material is between 80 wt% to 95 wt% of the composition.
16. The composition of claim 15, wherein the tobacco material is between 90 wt% to 95 wt% of the composition.
17. The composition of any of the preceding claims, further comprising water, wherein the water is between 5 wt% to 60 wt% of the composition.
18. The composition of claim 17, wherein the water is between 5 wt% to 40 wt% of the composition.
19. The composition of claim 18, wherein the water is between 5 wt% to 30 wt% of the composition.
20. The composition of claim 19, wherein the water is between 5 wt% to 20 wt% of the composition.
21. The composition of claim 20, wherein the water is between 5 wt% to 15 wt% of the composition.
22. The composition of claim 17, wherein the water is between 10 wt% to 40 wt% of the composition.
23. The composition of claim 22, wherein the water is between 10 wt% to 30 wt% of the composition.
24. The composition of claim 23, wherein the water is between 10 wt% to 20 wt% of the composition.
25. The composition of claim 24, wherein the water is between 10 wt% to 15 wt% of the composition.
26. The composition of any of the preceding claims, further comprising a humectant, wherein the humectant is between 1 wt% to 40 wt% of the composition.
27. The composition of any of the preceding claims, wherein the hydrated ionic clay is an anionic layered alkaline clay.
28. The composition of any of the preceding claims, wherein the hydrated ionic clay comprises silicates.
29. The composition of any of the preceding claims, wherein the hydrated ionic clay comprises aluminates, titanates, and/or zirconates.
30. The composition of any of the preceding claims, wherein the hydrated ionic clay comprises phosphates.
31. The composition of any of the preceding claims, wherein the hydrated ionic clay comprises alkali and/or alkaline earth metal silicates.
32. The composition of any of the preceding claims, wherein the hydrated ionic clay comprises layered double hydroxides.
33. The composition of any of the preceding claims, wherein the hydrated ionic clay is a synthetic trioctahedral clay mineral.
34. The composition of any of the preceding claims, wherein the hydrated ionic clay is a synthetic phyllosilicate.
35. The composition of claim 34, wherein the synthetic phyllosilicate is a lithium magnesium sodium orthosilicate.
36. The composition of claim 35, wherein the synthetic phyllosilicate is an inorganic composition comprising hydrogen, lithium, magnesium, sodium, oxygen, and silicon.
37. The composition of claim 36, wherein the inorganic composition is dilithium;hexadecamagnesium;disodium;l,3,5,7-tetraoxido-2,4,6,8,9,10-hexaoxa-l,3,5,7- tetrasilatricyclo[3.3.1.13,7]decane;dodecahydroxide.
38. The composition of claim 37, wherein the hydrated ionic clay is Laponite.
39. The composition of any of the preceding claims, wherein the hydrated ionic clay is a gel forming grade.
40. The composition of any of claims 1 to 38, wherein the hydrated ionic clay is a sol forming grade.
41. The composition of any of the preceding claims, wherein the tobacco material is a pure tobacco or a tobacco blend.
42. The composition of any of the preceding claims, wherein the tobacco material is at least one of Burley, Virginia, Kasturi, Oriental, and combinations thereof.
43. The composition of any of the preceding claims, further comprising an organic acid.
44. The composition of any of the preceding claims, further comprising a flavoring agent.
45. A composition comprising: a hydrated ionic clay, a tobacco material, and water.
46. The composition of claim 45, wherein the hydrated ionic clay is between 1 wt% to 5 wt%, the tobacco material is between 20 wt% to 95 wt%, and the water is between 1 wt% to 50 wt% of the composition.
47. The composition of claim 45, wherein the hydrated ionic clay is between 1 wt% to 4 wt%, the tobacco material is between 50 wt% to 90 wt%, and the water is between 5 wt% to 40 wt% of the composition.
48. The composition of claim 45, wherein the hydrated ionic clay is between 1 wt% to 3 wt%,
the tobacco material is between 60 wt% to 90 wt%, and the water is between 5 wt% to 30 wt% of the composition.
49. The composition of claim 45, wherein the hydrated ionic clay is between 1 wt% to 3 wt%, the tobacco material is between 50 wt% to 90 wt%, and the water is between 10 wt% to 30 wt% of the composition.
50. The composition of any of claims 45 to 49, further comprising a humectant.
51. The composition any of claims 45 to 50, further comprising an organic acid.
52. The composition any of claims 45 to 51, further comprising a flavoring agent.
53. The composition of any of claims 45 to 52, wherein the hydrated ionic clay is a synthetic trioctahedral clay mineral.
54. The composition of any of claims 45 to 53, wherein the hydrated ionic clay is a synthetic phyllosilicate.
55. The composition of claim 54, wherein the synthetic phyllosilicate is a lithium magnesium sodium orthosilicate.
56. The composition of claim 55, wherein the synthetic phyllosilicate is an inorganic composition comprising hydrogen, lithium, magnesium, sodium, oxygen, and silicon.
57. The composition of claim 56, wherein the wherein the inorganic composition is dilithium;hexadecamagnesium;disodium;l,3,5,7-tetraoxido-2,4,6,8,9,10-hexaoxa-l,3,5,7- tetrasilatricyclo[3.3.1.13,7]decane;dodecahydroxide.
58. The composition of claim 57, wherein the hydrated ionic clay is Laponite.
59. A cartridge containing the composition of any one of the preceding claims.
60. A device comprising a heating element configured to heat the composition of any one of the preceding claims to deliver nicotine or a salt thereof to a user.
61. The device of claim 60, wherein said device is an electronic nicotine delivery system.
62. The device of claim 60, wherein said device is based on combustion or exothermic reactions.
63. A method of extracting nicotine from a tobacco material comprising: contacting tobacco material with a hydrated ionic clay to form a composition; and contacting the composition with a solvent to extract the nicotine from the tobacco material.
64. The method of claim 63, wherein the tobacco material is a pure tobacco or a tobacco blend.
65. The method of claim 63, wherein the tobacco material is at least one of Burley, Virginia, Kasturi, Oriental, and combinations thereof.
66. The method of any of claims 63 to 65, wherein the hydrated ionic clay is an anionic layered alkaline clay.
67. The method of any of claims 63 to 66, wherein the hydrated ionic clay comprises silicates.
68. The method of any of claims 63 to 67, wherein the hydrated ionic clay comprises aluminates, titanates and/or zirconates.
69. The method of any of claims 63 to 68, wherein the hydrated ionic clay comprises phosphates.
70. The method of any of claims 63 to 69, wherein the hydrated ionic clay comprises alkali and/or alkaline earth metal silicates.
71. The method of any of claims 63 to 70, wherein the hydrated ionic clay comprises layered double hydroxides.
72. The method of any of claims 63 to 71, wherein the hydrated ionic clay is a synthetic trioctahedral clay mineral.
73. The method of any of claims 63 to 72, wherein the hydrated ionic clay is a synthetic phyllosilicate.
74. The method of claim 73, wherein the synthetic phyllosilicate is a lithium magnesium sodium orthosilicate.
75. The method of claim 74, wherein the synthetic phyllosilicate is an inorganic composition comprising hydrogen, lithium, magnesium, sodium, oxygen, and silicon.
76. The method of claim 75, wherein the inorganic composition is dilithium;hexadecamagnesium;disodium;l,3,5,7-tetraoxido-2,4,6,8,9,10-hexaoxa-l,3,5,7- tetrasilatricyclo[3.3.1.13,7]decane;dodecahydroxide.
77. The method of any of claims 63 to 76, wherein the hydrated ionic clay is Laponite.
78. The method of any of claims 63 to 77, wherein the hydrated ionic clay is a gel forming grade.
79. The method of any of claims 63 to 77, wherein the hydrated ionic clay is a sol forming grade.
80. The method of any of claims 63 to 79, wherein the solvent is an organic solvent.
81. The method of any of claims 63 to 80, wherein the solvent is a humectant.
82. The method of any of claims 63 to 81, wherein the solvent contains water.
83. The method of claims 63 to 82, further comprising: grinding the tobacco material to form a powdered tobacco material.
84. The method of claim 83, wherein the powdered tobacco material having particle size in the range of 50 to 2000 microns.
85. The method of claim 84, wherein the powdered tobacco material having particle size in the range of 100 to 300 microns.
86. The method of any of claims 63 to 85, further comprising: mixing the hydrated ionic clay with a first amount of water to form a first dispersion.
87. The method of claim 86, wherein the first dispersion has a pH value of between 5 and 12.
88. The method of claim 87, wherein the first dispersion has a pH value of between 9 and 11.
89. The method of claim 88, wherein the first dispersion has a pH value of between 9 and 10.
90. The method of any of claims 86 to 89, wherein the first amount of water is heated.
91. The method of any of claims 86 to 90, wherein the first amount of water is heated to 60 °C ± 20 °C.
92. The method of any of claims 86 to 91, wherein mixing the hydrated ionic clay with the first amount of water includes stirring the first dispersion until uniform.
93. The method of any of claims 86 to 92, wherein contacting tobacco material with the hydrated ionic clay to form the composition comprises mixing the powdered tobacco material with the first dispersion to form a second dispersion.
94. The method of claim 93, wherein a ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion is greater than 1 to 1.
95. The method of claim 93, wherein a ratio of powdered tobacco material to the hydrated ionic clay in the second dispersion is greater than 2 to 1.
96. The method of claim 93, wherein mixing the powdered tobacco material with the first dispersion to form the second dispersion includes stirring the second dispersion until uniform.
97. The method of any of claims 93 to 96, further comprising: evaporating a portion of the first amount of water from the second dispersion to form a loose cake.
98. The method of claim 97, wherein evaporating the portion of the first amount of water from the second dispersion comprises heating the second dispersion.
99. The method of any of claims 97 and 98, wherein evaporating the portion of the first amount of water from the second dispersion comprises heating the second dispersion under a vacuum.
100. The method of any of claims 97 and 99, further comprising: compressing the loose cake to form a mass selected from the group consisting of a pellet, a sheet, a brick, a bead, a powder, a granulation, a free flowing powder, a plug, a cylinder, a porous rod, and combinations thereof.
101. The method of claim 100, further comprising: drying the mass.
102. The method of claim 101, wherein drying the mass includes air drying the mass.
103. The method of claim 101, wherein drying the mass includes heating the mass.
104. The method of claim 101, wherein drying the mass includes freeze drying of the mass.
105. The method of any of claims 63 to 104, wherein contacting the composition with the solvent to extract the nicotine from the tobacco material comprises immersing the mass a first solution including a glycol and a glycerol.
106. The method of claim 105, wherein the glycol is propylene glycol and the glycerol is a vegetable glycerin.
107. The method of claim 104, further comprising: adding a second amount of water to the first solution to form a second solution, the second solution containing the nicotine extracted from the mass.
108. The method of any of claims 63 and 107, wherein the second solution further comprises an organic acid.
109. The method of any of claims 63 and 107, wherein the second solution further comprises a flavoring agent.
110. The method of any of claims 63 and 107, wherein greater than 50 % of the nicotine is extracted from the mass after 6 hours.
111. The method of claim 111, wherein greater than 60 % of the nicotine is extracted from the mass after 24 hours.
112. The method of claim 111, wherein greater than 80 % of the nicotine is extracted from the mass after 24 hours.
113. A method of manufacturing a pellet containing a tobacco material comprising: grinding tobacco material to form a powdered tobacco material; mixing a hydrated ionic clay with a first amount of water to form a first dispersion; mixing the powdered tobacco material with the first dispersion to form a second dispersion; evaporating a portion of the first amount of water from the second dispersion to form a loose cake; and compressing the loose cake to form the pellet containing tobacco material.
114. A system, comprising: a cartridge containing a composition comprising
a hydrated ionic clay, and a powdered tobacco material; a device comprising a receptacle configured to receive the cartridge.
115. The system of claim 114, wherein the cartridge further contains water.
116. The system of claim 115, wherein the cartridge further contains a humectant.
117. The system of claim 116, wherein the cartridge further contains a flavorant.
118. The system of claim 117, wherein the cartridge further contains organic acids.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA3164639A CA3164639A1 (en) | 2019-12-20 | 2020-12-17 | Hydrated ionic clay and tobacco material compositions |
EP20839510.3A EP4076021A1 (en) | 2019-12-20 | 2020-12-17 | Hydrated ionic clay and tobacco material compositions |
US17/844,834 US20220324715A1 (en) | 2019-12-20 | 2022-06-21 | Hydrated Ionic Clay and Tobacco Material Compositions |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US201962951983P | 2019-12-20 | 2019-12-20 | |
US62/951,983 | 2019-12-20 |
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US17/844,834 Continuation US20220324715A1 (en) | 2019-12-20 | 2022-06-21 | Hydrated Ionic Clay and Tobacco Material Compositions |
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WO2021127162A1 true WO2021127162A1 (en) | 2021-06-24 |
Family
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PCT/US2020/065587 WO2021127162A1 (en) | 2019-12-20 | 2020-12-17 | Hydrated ionic clay and tobacco material compositions |
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US (1) | US20220324715A1 (en) |
EP (1) | EP4076021A1 (en) |
CA (1) | CA3164639A1 (en) |
WO (1) | WO2021127162A1 (en) |
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- 2020-12-17 WO PCT/US2020/065587 patent/WO2021127162A1/en unknown
- 2020-12-17 EP EP20839510.3A patent/EP4076021A1/en active Pending
- 2020-12-17 CA CA3164639A patent/CA3164639A1/en active Pending
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CA622523A (en) * | 1961-06-20 | Minerals And Chemicals Corporation Of America | Tobacco composition and smoking unit containing material for eliminating deleterious matter | |
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US20220324715A1 (en) | 2022-10-13 |
EP4076021A1 (en) | 2022-10-26 |
CA3164639A1 (en) | 2021-06-24 |
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